Method for producing titanium compounds and compounds of nitrogen



Patented Dec. 8, 1931 g,ma as moan vonnrcsowsxit, or'or LnNnALn,CALIFORNIA; A ssIGNoa To TITAnIA oonroRA- TION, or LOS anennns,cAmronnIA;A- ooRPonATIon or oALIroamA 5 covery of the nitrogen of thetitanium com PATENT OFFICE H 1 METHOD non rnonuome TITANIUM ooiar'ounnsoomrounn's' on NITROGEN No Drawing.

The present invention relates to a method for producing titaniumcompounds and especially to the production of oxygen containing titaniumcompounds together with the re pounds in the form of combined nitrogen.

I have described, in my United States Letters Patent Number 1,7 42,67 4dated anuary 7 1930, the preparation of titanium oxide in from titaniumnitride by acting upon the latterwith nitric acid. In another pendingapplication for patent Serial No. 320,762 filed November 20th, 1928, Idescribe the acting upon titanium nitride with nitric acid in thepresence of sulphuric acid and show that from this reaction thereresults titanium acid sulphates. In the practicing of these discoveries,however, only a fraction of the nitride nitrogen of the titanium nitrideis recoverable as ammonia or in other combined form.

I have now found that by acting upon tivery good yield, are formed fromthe nitride nitrogen of the titanium nitride or cyanonitride.

As an example: One heats together titanium nitride and a per centsolution of perchloric acid. Dense fumesare soon given 0E. When thereaction is over the resulting white pasty mass, upon washing withwater, gives as a residue titanium dioxidewhile the wash water containsammonium compounds. The recovery of the nitrogen of the nitride in theform of ammonium perchlorate, ammonium chlorate, etc., is practicallyquantitative.

As a further example of my discovery: If one warms together titaniumnitride and a mixture of diluted sulphuric acid (sp. g. 1.40) and strongperchloric acid (sp. g. 1.5&) in excess of the theory one obtains asolution of Application filed October 30, 1929. Serial No. 403,660.

acid titanium sulphate and. ammonium .sul-

phate. The yields I are nearly quantitative. If desired one mayfurther'dilutesuch a solution, filter, pass in sulphur dioxide, and warmfor some hours atabout- 0., whereupon one obtains pure titanium oxide.The solution after filtering off the TiO may be worked up for therecovery of the ammonium compounds present. y I 3 Y If one.uses,'instead of perchloricjacid, a solution of sodium. or calciumhypochlorite in the presence of-hydrochloricacid or even solutions ofchlorinein water, either with-or without phosphoric acid-or phosphates,one

canobtain, fro1n-.titaniumnitride, ammonium salts and titanium dioxideOne may also use the ha1ates,perhalates or hypohalites of'other alkalior alkaline earth metals... It is further evident that these oxygenatedhalogensaltslor their acids may be produced: electrolytically in thepresence of :titanium nitride, water and a freeacid.

.1. Asan example: If anaqueous solution of sodium chloride, in which issuspended titaniumnitride and containing a little hydrochloric' acid,beelectrolyzed, in asuitable cell, one obtains titanium oxide and ammoniumsalts; -i a I It isto be understood that I do not confine my inventionto the examples as given .for they may be modified iby oneskilled in theart without departingfrom the scope of his invention. I I 5:

:What I claim as new and desire to secure by Letters-Patent is:

1.- .Method for the production. of titanium compounds containing oxygenby acting upon titanium nitrogenv compounds with halogen compoundshavingv an oxidizing action and in the presence of water and a' freeacid and recovering the nitrogenoffthe titanium nitrogen compound in acombined form. r

2.. Method for the production oftitanium compounds containing oxygenandespecially titanium acid sulphates by acting upon titanium nitrogencompounds with oxidizing halogen'compounds in the presence ofwater andsulphuric acid and recovering the nitrogenof the titanium nitrogencompound in a. combined form. I

loo

um nitride with by ochlorous acid in the presence of sulphuric acid andwater and recovering the nitrogen of the titanium nitride as ammoniumsulphate.

12. Method for the production of titanium oxide by acting upon titaniumnitride with hypochlorous acid in the presence of water and sodiumphosphate.

, FOORD VON BICHOWSKY.

nitrogen-compounds with a hypochlorite of an alkaline metal in thepresence of water and a halogen acid andyrecovering the nitrogen of thetitanium nitrogen compound as anammonium compound.

' 5. Method forthegproductionof titanium compounds" containing oxygenand especially titanium dioxide by acting upon'titanium nitrogencompounds with "a' chlorate of an alkaline metal in the presence ofwater and a halogen acid and recovering the nitrogen of the'tita-niumnitrogen compound as an ammonium compound.

'6. 'Method "forlitlie .product-ionof titanium compoundscontaining'oxygen and especially titanium dioxide by acting upontitanium nit-rogen com-pounds 'with a perchlorate of an alkaline metalin the presence of water and a halogen acid and recovering the'nitrogenof the titanlu-m nitrogen compound asan ammonium compound. I e

7. Method for thepro'duction oftit-anium compounds containing oxygen andespecially titanium acid-sulphate by acting upon titan ium nitrogencompounds with hypoc'hlo i v rous acid in the presence of water andsulphuric acid and recovering the nitrogen of the titanium nitrogencompoundas ammonium sulphate. f 3

I '8 Method for the production of titanium compounds containing oxygenand especially titanium acid sulphate by acting upontitanium nitrogencompounds with chloric acid inthe presence of water-and sulphuric acidand recovering the nitrogen of the titanium nitrogen compound asammonium sulphate.

9. Method for the production of titanium compounds containing oxygen andespecially titanium acid sulphate by acting upon titanium nitrogencompounds-with perchloric acidin the presence of water and sulphuricacid'and recovering the nitrogen of the titanium nitrogen compound asammonium sulphate. 19. Method fortheproduction of titanium compoundscontaining oxygen and especially sodium titanium acid sulphate by actingupon titanium nitride and sulphuric acidwith an aqueous solution ofsodium hypochlorite and "recovering the nitrogen of the titanium ni--tride'in the form of ammonium sulphate.

11. Methodfor the production of titanium compounds containing oxygen andespecially titanium acid sulphate by acting upon titani-

